Potassium Iodide → N-(2,6-difluoropyridin-3-yl)-N-(2-oxopropyl)formamide

HRID 546781노트

반응식

HRID 546781 반응식
Cl[CH2:2][C:3](=[O:5])[CH3:4].C(=O)([O-])[O-].[Cs+].[Cs+].[I-].[K+].[F:14][C:15]1[C:20]([NH:21][CH:22]=[O:23])=[CH:19][CH:18]=[C:17]([F:24])[N:16]=1>CN(C)C=O.O.C(OCC)(=O)C>[F:14][C:15]1[C:20]([N:21]([CH2:2][C:3](=[O:5])[CH3:4])[CH:22]=[O:23])=[CH:19][CH:18]=[C:17]([F:24])[N:16]=1

참가 물질

8

반응물 4

HCID 4875Potassium IodideHCID 6571ChloroacetoneHCID 10796Cesium carbonateHCID 86628515N-(2,6-difluoropyridin-3-yl)formamide

생성물 1

HCID 86628516N-(2,6-difluoropyridin-3-yl)-N-(2-oxopropyl)formamide

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

Chloroacetone (1.83 ml), cesium carbonate (7.99 g) and potassium iodide (254 mg) were added to a solution of N-(2,6-difluoropyridin-3-yl)formamide (2.42 g) in N,N-dimethylformamide (50 ml), and the reaction solution was stirred at room temperature for two hours. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and then the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (2.52 g). The property values of the compound are as follows.

후처리

  1. customthe organic layer was separated
  2. washThe resulting organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe drying agent was separated by filtration
  5. concentrationthe organic layer was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-cfc561bdf5c74c69baf3294907009449
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935815B2

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